AT403043B - METHOD FOR THE CONTINUOUS PRODUCTION OF FALLED CALCIUM CARBONATE - Google Patents

METHOD FOR THE CONTINUOUS PRODUCTION OF FALLED CALCIUM CARBONATE Download PDF

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Publication number
AT403043B
AT403043B AT0059896A AT59896A AT403043B AT 403043 B AT403043 B AT 403043B AT 0059896 A AT0059896 A AT 0059896A AT 59896 A AT59896 A AT 59896A AT 403043 B AT403043 B AT 403043B
Authority
AT
Austria
Prior art keywords
gas
hydrate
cell
calcium carbonate
slurry
Prior art date
Application number
AT0059896A
Other languages
German (de)
Other versions
ATA59896A (en
Original Assignee
Unitechnik Thurner Anlagenbaug
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Unitechnik Thurner Anlagenbaug filed Critical Unitechnik Thurner Anlagenbaug
Priority to AT0059896A priority Critical patent/AT403043B/en
Priority to EP96112476A priority patent/EP0799797B1/en
Priority to DE59601499T priority patent/DE59601499D1/en
Priority to ES96112476T priority patent/ES2131895T3/en
Publication of ATA59896A publication Critical patent/ATA59896A/en
Priority to CZ97887A priority patent/CZ88797A3/en
Priority to SK409-97A priority patent/SK40997A3/en
Priority to HRA598/96A priority patent/HRP970181B1/en
Priority to HU9700696A priority patent/HUP9700696A1/en
Application granted granted Critical
Publication of AT403043B publication Critical patent/AT403043B/en
Priority to GR990401626T priority patent/GR3030549T3/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/18Carbonates
    • C01F11/181Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Treating Waste Gases (AREA)

Claims (4)

AT 403 043 B Die Erfindung bezieht sich auf die Kontinuierliche Herstellung eines Weißpigmentes (Kalziumkarbonat) unter Verwendung von Kalziumhydrat und Kohlendioxidgas, entsprechend der Formel Ca(OH)z + C02_CaC03 + H20 Der bisherige Stand der Technik beschränkt sich auf die Mahlung natürlichen Karbonates (Marmor, Kreide) bzw. auf Erfindungen zur Herstellung von gefälltem Kalziumkarbonat in chargenweisen Prozessen. Ein weiteres Verfahren stellt stufenweise gefälltes Kalziumkarbonat her, indem eine nieder konzentrierte, wäßrige Kalziumhydrat-Suspension in einen CO2 Gasstrom, welcher sich innerhalb der hintereinander geschalteten Sprühtürme befindet, gesprüht wird. Die technische Aufgabe, mit welcher die Erfindung zur kontinuierlichen Herstellung gelöst wird, ist gekennzeichnet durch ein Verfahren der fortschreitenden Karbonisierung in seriell geschalteten Zellen, bis zur Erreichung eines stabilen Kalziumkarbonates, wobei die Zuführung von Gas und Slurry sowie deren Dispergierung (Figur 1) in der Weise erfolgt, daß je Zelle eine Gas- (2) und Slurryzufuhreinrichtung (1) mit integriertem Rührwerk (RW) vorgesehen ist. Ein ebenso entscheidender Teil der Erfindung ist die Ausführung der Einrichtung zur Dispergierung des Kalziumhydrates mit dem CO2 des Rauchgases. Zur umfassenden industriellen Verwendung des präzipitierten Kalziumkarbonates (PCC) ist neben der Stabilität auch die Erreichung gewünschter Korngrößen und deren Verteilung, sowie die Herstellung bestimmter Kristallformen von besonderer Bedeutung. Das Verfahren erlaubt die Herstellung der von den Anwendern vorwiegend geforderten Kristallformen: Kalzit - rhombohedral und scaienohedral Aragonit - acicular Kalzit erfordert, wie aus der Literatur bekannt, Reaktionstemperaturen unter 30 * C, wobei der scalenohedrale Kalzit bei Temperaturen von 25-28’C und der rhombohedrale Kalzit nur bei sehr niederen Temperaturen entsteht. Aragonit benötigt höhere Temperaturen, vorzugsweise 30-36 *C. Eine Beschleunigung der Startzeiten wird dadurch erreicht, daß die erste Zelle mit Karbonat der angestrebten Kristallform zu 2/3 gefüllt und mit Beginn des Hydratdurchflusses sofort das Rauchgas eingeleitet wird. Die Karbonisierung gelingt schon ab einer C02 Konzentration im Rauchgas von 10%. Die Leistung der Zellblöcke ist proportional der C02 Konzentration. Die Korngröße wird von der Konzentration der Hydratsuspension, der Durchflußmenge und dem Rauchgasüberschuß beeinflußt. Die hier beanspruchte Erfindung, dargestellt in Fig.1, besteht - je nach gewünschter Leistung - aus einem bis mehreren Blöcken mit quadratischen Zellen mit wenigstens 340 Liter Inhalt je Zelle. Jede Zelle ist mit einem speziellen Rührwerk zur Dispergierung des Hydratslurrys mit dem Rauchgas ausgestattet. Dazu ist ein offenes, kombiniertes Gas- und Slurryrohr über der Rührwerkswelle am Motor zentrisch angeflanscht. Das Rührorgan erzeugt einen bestimmten Unterdrück, der einerseits die Einbringung des Gases (2) unter minimalem Druck erlaubt und andererseits die Zirkulation innerhalb der Zelle verstärkt. Diese Kombination ergibt eine Dispergierung, welche die Reaktion zwischen Hydrat und Gas bei kleinster Rührwerksleistung (1,5 kW) ermöglicht. Das Hydrat gelangt von einer Zelle (3) über ein geneigtes Rohr (1,4) drucklos in das kombinierte Gas- und Slurryrohr (2) der nächsten Zelle. Die Karbonisierung wird über die Rauchgas- bzw. Durchflußmenge, sowie die eingestellte Konzentration der Hydratsuspension gesteuert. Patentansprüche 1. Verfahren zur kontinuierlichen Erzeugung von gefälltem Kalziumkarbonat, dadurch gekennzeichnet, daß die Karbonisierung in seriell geschalteten Zellen erfolgt, wobei die Zuführung von Gas und Slurry sowie deren Dispergierung (Figur 1) in der Weise erfolgt, daß je Zelle eine Gas- (2) und Slurryzufuhreinrichtung (1) mit integriertem Rührwerk (RW) vorgesehen ist.AT 403 043 B The invention relates to the continuous production of a white pigment (calcium carbonate) using calcium hydrate and carbon dioxide gas, according to the formula Ca (OH) z + C02_CaC03 + H20. The previous state of the art was limited to the grinding of natural carbonates (marble , Chalk) or inventions for the production of precipitated calcium carbonate in batch processes. Another method produces stepwise precipitated calcium carbonate by spraying a low-concentration, aqueous calcium hydrate suspension into a CO2 gas stream, which is located within the spray towers connected in series. The technical problem with which the invention is solved for continuous production is characterized by a process of progressive carbonization in series-connected cells until a stable calcium carbonate is reached, the supply of gas and slurry and their dispersion (FIG. 1) in the In this way, one gas (2) and one slurry feed device (1) with an integrated agitator (RW) is provided for each cell. An equally crucial part of the invention is the implementation of the device for dispersing the calcium hydrate with the CO2 of the flue gas. For the extensive industrial use of the precipitated calcium carbonate (PCC), in addition to stability, the achievement of desired grain sizes and their distribution, as well as the production of certain crystal forms, are of particular importance. The method allows the production of the crystal forms that are mainly required by the users: calcite - rhombohedral and scaienohedral aragonite - acicular calcite requires, as known from the literature, reaction temperatures below 30 ° C, the scalenohedral calcite at temperatures of 25-28'C and rhombohedral calcite only occurs at very low temperatures. Aragonite needs higher temperatures, preferably 30-36 * C. Acceleration of the start times is achieved by filling the first cell 2/3 with carbonate of the desired crystal shape and immediately introducing the flue gas as the hydrate flow begins. Carbonation is possible from a CO 2 concentration in the flue gas of 10%. The performance of the cell blocks is proportional to the C02 concentration. The grain size is influenced by the concentration of the hydrate suspension, the flow rate and the flue gas excess. The invention claimed here, shown in Fig.1, consists - depending on the desired performance - of one to several blocks with square cells with at least 340 liters of content per cell. Each cell is equipped with a special agitator for dispersing the hydrate slurry with the flue gas. For this purpose, an open, combined gas and slurry tube is flanged centrally over the agitator shaft on the motor. The stirring element generates a certain negative pressure, which on the one hand allows the introduction of gas (2) under minimal pressure and on the other hand increases the circulation within the cell. This combination results in a dispersion that enables the reaction between hydrate and gas with the lowest agitator output (1.5 kW). The hydrate passes from a cell (3) via an inclined pipe (1,4) without pressure into the combined gas and slurry pipe (2) of the next cell. The carbonization is controlled via the flue gas or flow rate, as well as the concentration of the hydrate suspension. 1. Process for the continuous production of precipitated calcium carbonate, characterized in that the carbonization takes place in series-connected cells, the supply of gas and slurry and their dispersion (Figure 1) in such a way that one gas (2 ) and slurry feed device (1) with an integrated agitator (RW) is provided. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß Zellen eingesetzt werden, deren Größe mindestens 700 x 700 x 1000 mm betragt.2. The method according to claim 1, characterized in that cells are used whose size is at least 700 x 700 x 1000 mm. 3. Verfahren nach den Ansprüchen 1 und 2, dadurch gekennzeichnet, daß eine Blockanordnung der Zellen vorgesehen ist, wobei sich die Anzahl der Zellen und Blöcke durch die Anlagenkapazität ergibt. 2 AT 403 043 B3. The method according to claims 1 and 2, characterized in that a block arrangement of the cells is provided, the number of cells and blocks resulting from the system capacity. 2 AT 403 043 B 4. Verfahren nach den Ansprüchen 1 bis 3, dadurch gekennzeichnet, daß scalenohedraler Kalzit bei Temperaturen von unter 28 "C, rhombohedraler Kalzit bei Temperaturen von unter 15 °C, acicularer Aragonit bei Temperaturen von über 30 · C hergestellt wird. Hiezu 1 Blatt Zeichnungen 34. Process according to claims 1 to 3, characterized in that scalenohedral calcite is produced at temperatures below 28 ° C, rhombohedral calcite at temperatures below 15 ° C, acicular aragonite at temperatures above 30 ° C. With 1 sheet of drawings 3
AT0059896A 1996-04-03 1996-04-03 METHOD FOR THE CONTINUOUS PRODUCTION OF FALLED CALCIUM CARBONATE AT403043B (en)

Priority Applications (9)

Application Number Priority Date Filing Date Title
AT0059896A AT403043B (en) 1996-04-03 1996-04-03 METHOD FOR THE CONTINUOUS PRODUCTION OF FALLED CALCIUM CARBONATE
EP96112476A EP0799797B1 (en) 1996-04-03 1996-08-02 Continuous process for the production of precipitated calcium carbonate
DE59601499T DE59601499D1 (en) 1996-04-03 1996-08-02 Continuous process for the production of precipitated calcium carbonate
ES96112476T ES2131895T3 (en) 1996-04-03 1996-08-02 PROCEDURE FOR THE PRODUCTION OF PRECIPITATED CALCIUM CARBONATE.
CZ97887A CZ88797A3 (en) 1996-04-03 1997-03-24 Process of continuous preparation of precipitated calcium carbonate
SK409-97A SK40997A3 (en) 1996-04-03 1997-03-26 Method for the continuous production of precipitated calcium carbonate
HRA598/96A HRP970181B1 (en) 1996-04-03 1997-04-02 Continuous process for the production of precipitated calcium carbonate
HU9700696A HUP9700696A1 (en) 1996-04-03 1997-04-03 Method for continous producing precipitated chalk
GR990401626T GR3030549T3 (en) 1996-04-03 1999-06-16 Continuous process for the production of precipitated calcium carbonate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
AT0059896A AT403043B (en) 1996-04-03 1996-04-03 METHOD FOR THE CONTINUOUS PRODUCTION OF FALLED CALCIUM CARBONATE

Publications (2)

Publication Number Publication Date
ATA59896A ATA59896A (en) 1997-03-15
AT403043B true AT403043B (en) 1997-10-27

Family

ID=3494827

Family Applications (1)

Application Number Title Priority Date Filing Date
AT0059896A AT403043B (en) 1996-04-03 1996-04-03 METHOD FOR THE CONTINUOUS PRODUCTION OF FALLED CALCIUM CARBONATE

Country Status (9)

Country Link
EP (1) EP0799797B1 (en)
AT (1) AT403043B (en)
CZ (1) CZ88797A3 (en)
DE (1) DE59601499D1 (en)
ES (1) ES2131895T3 (en)
GR (1) GR3030549T3 (en)
HR (1) HRP970181B1 (en)
HU (1) HUP9700696A1 (en)
SK (1) SK40997A3 (en)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9802999D0 (en) * 1998-02-13 1998-04-08 Ecc Int Ltd Production of products containing precipitated calcium carbonate
US6451268B1 (en) 1999-04-16 2002-09-17 Minerals Technologies Inc. Method and apparatus for continuous gas liquid reactions
DE19943093A1 (en) * 1999-09-09 2001-03-15 Solvay Soda Deutschland Gmbh Process for the continuous production of precipitated calcium carbonate
US6355138B1 (en) 2000-02-24 2002-03-12 Voith Sulzer Paper Technology North America, Inc. Method of chemically loading fibers in a fiber suspension
US6533895B1 (en) 2000-02-24 2003-03-18 Voith Sulzer Paper Technology North America, Inc. Apparatus and method for chemically loading fibers in a fiber suspension
DE10120635A1 (en) * 2001-04-27 2002-10-31 Voith Paper Patent Gmbh Method and device for loading fibers with calcium carbonate
BRPI0601717A (en) * 2006-05-04 2007-12-18 Du Pont Brasil process for the manufacture of calcium carbonate
US8445217B2 (en) 2007-09-20 2013-05-21 Vanderbilt University Free solution measurement of molecular interactions by backscattering interferometry
WO2011156713A1 (en) 2010-06-11 2011-12-15 Vanderbilt University Multiplexed interferometric detection system and method
US9562853B2 (en) 2011-02-22 2017-02-07 Vanderbilt University Nonaqueous backscattering interferometric methods
PL2599750T3 (en) 2011-11-29 2015-03-31 Hf Biotec Berlin Gmbh Method and assembly for semi-continuous manufacture of crystalline calcium carbonate
US9273949B2 (en) 2012-05-11 2016-03-01 Vanderbilt University Backscattering interferometric methods
EP3247988A4 (en) 2015-01-23 2018-12-19 Vanderbilt University A robust interferometer and methods of using same
US10627396B2 (en) 2016-01-29 2020-04-21 Vanderbilt University Free-solution response function interferometry

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2739704B2 (en) * 1976-10-01 1979-06-07 Shiraishi Kogyo Kaisha, Ltd., Amagasaki, Hyogo (Japan) Process for the production of cubic calcium carbonate crystals
DE2742829B2 (en) * 1976-09-25 1979-10-31 Shiraishi Kogyo Kaisha, Ltd., Amagasaki, Hyogo (Japan) Process for the continuous production of precipitated calcium carbonate
GB2023561A (en) * 1978-04-05 1980-01-03 Shiraishi Kogyo Kaisha Ltd Calcium carbonate

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3150926A (en) * 1961-05-15 1964-09-29 Champion Papers Inc Fluidized production of calcium carbonate
US4888160A (en) * 1985-12-20 1989-12-19 J.M. Huber Corporation Process for producing calcium carbonate and products thereof
US4824654A (en) * 1988-03-17 1989-04-25 Yabashi Industries Co., Ltd. Process of producing needle-shaped calcium carbonate particles
EP0429707B1 (en) * 1989-11-29 1996-03-27 SCHAEFER KALK Kommanditgesellschaft Process for the preparation of basic calcium carbonate, basic calcium carbonate therefrom and its use
GB2248229B (en) * 1990-09-27 1994-10-26 Ecc Int Ltd Precipitated calcium carbonate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2742829B2 (en) * 1976-09-25 1979-10-31 Shiraishi Kogyo Kaisha, Ltd., Amagasaki, Hyogo (Japan) Process for the continuous production of precipitated calcium carbonate
DE2759551B1 (en) * 1976-09-25 1981-02-19 Shiraishi Kogyo Kaisha Ltd Process for the continuous production of precipitated calcium carbonate
DE2739704B2 (en) * 1976-10-01 1979-06-07 Shiraishi Kogyo Kaisha, Ltd., Amagasaki, Hyogo (Japan) Process for the production of cubic calcium carbonate crystals
GB2023561A (en) * 1978-04-05 1980-01-03 Shiraishi Kogyo Kaisha Ltd Calcium carbonate

Also Published As

Publication number Publication date
GR3030549T3 (en) 1999-10-29
HUP9700696A1 (en) 2000-05-28
HU9700696D0 (en) 1997-05-28
HRP970181A2 (en) 1998-04-30
ATA59896A (en) 1997-03-15
ES2131895T3 (en) 1999-08-01
EP0799797B1 (en) 1999-03-24
EP0799797A1 (en) 1997-10-08
HRP970181B1 (en) 2000-04-30
DE59601499D1 (en) 1999-04-29
CZ88797A3 (en) 1997-10-15
SK40997A3 (en) 1997-11-05

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EELA Cancelled due to lapse of time